CN109133031A - A kind of preparation method of porous carbon microsphere electrode material for super capacitor - Google Patents

A kind of preparation method of porous carbon microsphere electrode material for super capacitor Download PDF

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Publication number
CN109133031A
CN109133031A CN201811201119.XA CN201811201119A CN109133031A CN 109133031 A CN109133031 A CN 109133031A CN 201811201119 A CN201811201119 A CN 201811201119A CN 109133031 A CN109133031 A CN 109133031A
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China
Prior art keywords
porous carbon
carbon microsphere
super capacitor
preparation
electrode material
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CN201811201119.XA
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Chinese (zh)
Inventor
余建国
李瑶
刘林
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Tianjin Polytechnic University
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Tianjin Polytechnic University
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Priority to CN201811201119.XA priority Critical patent/CN109133031A/en
Publication of CN109133031A publication Critical patent/CN109133031A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/05Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/24Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/32Carbon-based
    • H01G11/42Powders or particles, e.g. composition thereof
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/30Particle morphology extending in three dimensions
    • C01P2004/32Spheres
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/61Micrometer sized, i.e. from 1-100 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/12Surface area
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Power Engineering (AREA)
  • Materials Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Electric Double-Layer Capacitors Or The Like (AREA)

Abstract

The present invention is made from starch; after aluminum potassium sulfate solution pre-processes; it is carbonized in nitrogen; it is cooling; neutrality is washed with distilled water to after dilute hydrochloric acid pickling; porous carbon microsphere is obtained after filtration drying, the synthetic method is simple and is easy to large-scale production, and synthesized porous carbon microsphere has good performance of the supercapacitor.

Description

A kind of preparation method of porous carbon microsphere electrode material for super capacitor
Technical field
The present invention relates to electrode material for super capacitor preparation fields, and in particular to a kind of preparation side of porous carbon microsphere Method.
Background technique
Supercapacitor is due to its high power density, the unique properties such as fast charging and discharging rate and excellent cyclical stability And more and more concerns are caused as novel energy storage device in scientific research.In general, the electrification of supercapacitor It learns performance and is substantially dependent on electrode material, porous carbon is most common electrode material for super capacitor, because its surface area is big, electricity Sub- conductivity is high, and aperture is adjustable, and chemical stability is splendid, advantage of lower cost and be concerned.Recently, researcher is dedicated to Various forms of novel porous carbon are developed, high-performance super capacitor, such as graded porous carbon, template carbon, carbon ball, carbide are used for Derived carbon, carbon nanotube and graphene.
Recently, porous carbon ball shows the prospect for advanced energy-storage system.The geometry of their rules, adjustable diameter Effective method is provided with aperture to customize excellent chemical property.In addition, closely packed carbon ball provides hole between ball Degree buffers reservoir as ion, is conducive to fast ionic diffusion and transports internal carbon surface, to improve the electrochemistry of material Performance.In addition, mixing hetero atom such as oxygen, nitrogen etc. in carbon structure helps to improve the electricity and chemical property of carbon surface.
The preparation method of carbon ball mainly includes activation method, template, hydro-thermal method, chemical vapour deposition technique, carbonization gel method Deng the most commonly used is template, the present invention is using cheap cornstarch as carbon source.A kind of no template in-situ activation is developed to be formed Porous carbon microsphere.
Summary of the invention
The present invention is with template-free method one-step synthesis porous carbon microsphere.
Technical scheme is as follows:
The 12 hydrazine aluminum sulfate potassium for weighing certain mass are placed in 100 milliliters of ultrapure waters, and stirring clarifies to be formed to solution Aluminum potassium sulfate solution weighs 3 grams of starch and is placed in aluminum potassium sulfate solution, the filtration drying after soaking at room temperature 24 hours, dry Sample afterwards, which is put into tube furnace, is warming up to 800~1000 DEG C under nitrogen atmosphere, keep the temperature 4 hours, cooling, 2mol/L chlorohydric acid pickling After be washed with distilled water to neutrality, obtain porous carbon microsphere after filtration drying.
Porous carbon ball material synthesized by the present invention is made into electrode of super capacitor, tests its performance of the supercapacitor.
The concentration of heretofore described aluminum aluminum sulfate are as follows: 0.126~0.190mol/L.
The preparation method of heretofore described porous carbon microsphere is simply easy to large-scale production.
Detailed description of the invention
Fig. 1 is scanning electron microscope (SEM) picture of the porous carbon microsphere prepared in embodiment 1;
Fig. 2 is scanning electron microscope (SEM) picture of the porous carbon microsphere prepared in embodiment 2;
Fig. 3 is that adsorption curve is desorbed in the porous carbon microsphere nitrogen prepared in embodiment 1;
Fig. 4 is that adsorption curve is desorbed in the porous carbon microsphere nitrogen prepared in embodiment 2;
Fig. 5 is the charging and discharging curve figure of the porous carbon microsphere for preparing at 1~20A/g of current density in embodiment 1.
Fig. 6 is the charging and discharging curve figure of the porous carbon microsphere for preparing at 1~20A/g of current density in embodiment 2.
Specific embodiment
Embodiment 1
It weighs 3 grams of starch to be placed in the aluminum potassium sulfate solution of 100 milliliters of 0.126mol/L, soaking at room temperature filters after 24 hours It is dry, the sample after drying is put into tube furnace and is warming up to 800 DEG C, constant temperature 4h under nitrogen atmosphere, cooling, 2mol/L hydrochloric acid acid It is washed with distilled water to neutrality after washing, obtains porous carbon microsphere after filtration drying.Attached drawing 1 shows prepared carbon material in ball Shape, Fig. 3 show that the carbosphere has pore structure abundant, the specific surface area of carbosphere are as follows: 979.08m2g-1;It should shown in Fig. 5 The maximum specific capacitance of material is 174F/g.
Embodiment 2
It weighs 3 grams of starch to be placed in the aluminum potassium sulfate solution of 100 milliliters of 0.190mol/L, soaking at room temperature filters after 24 hours It is dry, the sample after drying is put into tube furnace and is warming up to 800 DEG C under nitrogen atmosphere, constant temperature 4 hours, cooling, 2mol/L salt It is washed with distilled water to neutrality after pickling, obtains porous carbon microsphere after filtration drying.Attached drawing 1 shows that prepared carbon material is in Spherical shape, Fig. 4 show that the carbosphere has pore structure abundant, the specific surface area of carbosphere are as follows: 1052.70m2g-1;Shown in Fig. 6 The maximum specific capacitance of the material is 196F/g.

Claims (4)

1. a kind of preparation method of porous carbon microsphere electrode material for super capacitor, which is characterized in that weigh 3 grams of starch and be placed in In 100 milliliters of certain density aluminum potassium sulfate solutions, the sample after drying is put into pipe by filtration drying after soaking at room temperature 24 hours High-temperature calcination under nitrogen atmosphere in formula furnace, it is constant temperature 4 hours, cooling, it is washed with distilled water to after 2mol/L hydrochloric acid solution pickling Property obtains porous carbon microsphere after filtration drying.
2. a kind of preparation method of porous carbon microsphere electrode material for super capacitor, feature according to claims 1 exist In the concentration range of the aluminum potassium sulfate solution are as follows: 0.126~0.190mol/L.
3. a kind of preparation method of porous carbon microsphere electrode material for super capacitor, feature according to claims 1 exist In the high-temperature calcination temperature be 800~1000 DEG C.
4. porous carbon microsphere material synthesized by claims 1 is made into electrode of super capacitor, its supercapacitor is tested Performance, maximum specific capacity reach 196F/g.
CN201811201119.XA 2018-10-15 2018-10-15 A kind of preparation method of porous carbon microsphere electrode material for super capacitor Pending CN109133031A (en)

Priority Applications (1)

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CN201811201119.XA CN109133031A (en) 2018-10-15 2018-10-15 A kind of preparation method of porous carbon microsphere electrode material for super capacitor

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Application Number Priority Date Filing Date Title
CN201811201119.XA CN109133031A (en) 2018-10-15 2018-10-15 A kind of preparation method of porous carbon microsphere electrode material for super capacitor

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CN109133031A true CN109133031A (en) 2019-01-04

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110330014A (en) * 2019-07-16 2019-10-15 兰州理工大学 The preparation method of starch porous carbon microsphere for electrode material for super capacitor
CN112194123A (en) * 2020-10-20 2021-01-08 福州大学 Low-cost porous carbon microsphere and preparation method thereof
CN116041989A (en) * 2023-01-10 2023-05-02 聚能新材料科技(荆门)有限公司 Biomass carbon sphere, preparation method thereof, antistatic composite material and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104045074A (en) * 2014-06-18 2014-09-17 广西师范大学 Starch-based hollow porous carbon microsphere and preparation method thereof
CN104445149A (en) * 2014-11-25 2015-03-25 天津工业大学 Method for preparing hollow carbon microspheres with high oxygen content

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104045074A (en) * 2014-06-18 2014-09-17 广西师范大学 Starch-based hollow porous carbon microsphere and preparation method thereof
CN104445149A (en) * 2014-11-25 2015-03-25 天津工业大学 Method for preparing hollow carbon microspheres with high oxygen content

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110330014A (en) * 2019-07-16 2019-10-15 兰州理工大学 The preparation method of starch porous carbon microsphere for electrode material for super capacitor
CN110330014B (en) * 2019-07-16 2022-07-08 兰州理工大学 Preparation method of starch porous carbon microspheres for supercapacitor electrode material
CN112194123A (en) * 2020-10-20 2021-01-08 福州大学 Low-cost porous carbon microsphere and preparation method thereof
CN116041989A (en) * 2023-01-10 2023-05-02 聚能新材料科技(荆门)有限公司 Biomass carbon sphere, preparation method thereof, antistatic composite material and preparation method thereof

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Application publication date: 20190104